CN117701124A - Silane modified polyether waterproof coating and preparation method and application thereof - Google Patents

Silane modified polyether waterproof coating and preparation method and application thereof Download PDF

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CN117701124A
CN117701124A CN202311668605.3A CN202311668605A CN117701124A CN 117701124 A CN117701124 A CN 117701124A CN 202311668605 A CN202311668605 A CN 202311668605A CN 117701124 A CN117701124 A CN 117701124A
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silane
polyether
modified
parts
waterproof coating
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何宏林
宋方方
陈立义
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Keshun Waterproof Technology Co Ltd
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Keshun Waterproof Technology Co Ltd
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Priority to CN202311668605.3A priority Critical patent/CN117701124A/en
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Abstract

The application provides a silane modified polyether waterproof coating, a preparation method and application thereof, wherein the silane modified polyether waterproof coating comprises the following raw materials in parts by mass: modified alkoxysilane-terminated polyether: 100 parts of modified alkoxy silane end-capped polyether, wherein the modified alkoxy silane end-capped polyether comprises an amino group, and the amino group comprises a secondary amino group; alkoxysilane-terminated polyethers: 350-700 parts; the alkoxy silane end capped polyether does not contain amino; polyisocyanates: 7-16 parts; chain extender: 27-54 parts; and (3) a plasticizer: 500-800 parts; and (3) filling: 300-480 parts; coupling agent: 35-50 parts. The silane modified polyether waterproof coating has higher tearing strength, and is matched with conventional alkoxy silane end-capped polyether without amine groups and other assistants to ensure that the performances of tensile strength, elongation at break, low-temperature flexibility and the like meet the requirements.

Description

Silane modified polyether waterproof coating and preparation method and application thereof
Technical Field
The application relates to the technical field of waterproof coatings, in particular to a silane modified polyether waterproof coating and a preparation method and application thereof.
Background
The silane modified polyether waterproof coating is a single-component solvent-free waterproof coating which is prepared by taking silane modified polyether resin as a base polymer and adding functional additives, filler, pigment and catalyst, and has the advantages of high elongation, high tensile strength, good low-temperature flexibility and low water absorption. The silane modified polyether waterproof paint is mainly used for waterproof and moistureproof of kitchen, bathroom, balcony and the like, is coated on a base layer when in use, and is cured through reaction with moisture to form a continuous seamless high-molecular elastic waterproof film. The silane modified polyether waterproof paint can be used for roofing, external wall and other parts under the condition of applying a proper protective layer.
The tearing strength refers to the maximum tensile force which can be born by the material under the action of a force perpendicular to the surface of the material, and is generally used for measuring the anti-damage capability of the material, and is also an important factor for waterproof paint, and the tearing damage of the paint surface can lead to the water seepage of a coating film, so that the coating film can drop off and peel off in the use environment. Although the traditional silane modified polyether waterproof coating has higher elongation at break and higher tensile strength, the lower tearing strength of the traditional silane modified polyether waterproof coating greatly limits the popularization and application of the silane modified polyether waterproof coating.
Therefore, there is a need to provide a silane modified polyether waterproof coating with higher tear strength.
Disclosure of Invention
The application provides a silane modified polyether waterproof coating, a preparation method and application thereof, and a coating obtained by the silane modified polyether waterproof coating has higher tearing strength, thereby being beneficial to expanding the application scene of the silane modified polyether waterproof coating.
In a first aspect, the application provides a silane modified polyether waterproof coating, which comprises the following raw materials in parts by mass:
modified alkoxysilane-terminated polyether: 100 parts of modified alkoxy silane end capped polyether containing secondary amino;
alkoxysilane-terminated polyethers: 350-700 parts; the chain segment of the alkoxy silane group end capped polyether does not contain amino groups;
polyisocyanates: 7-16 parts;
chain extender: 27-54 parts;
and (3) a plasticizer: 500-800 parts;
and (3) filling: 300-480 parts;
coupling agent: 35-50 parts.
According to the application, in the silane modified polyether waterproof coating, the amino groups in the modified alkoxy silane group end capped polyether can provide active sites for reaction with polyisocyanate, so that the crosslinking density of the polymer in the coating can be increased, the tearing strength of the coating formed by the coating can be effectively improved, and meanwhile, the conventional alkoxy silane group end capped polyether without amino groups and other auxiliary agents are matched to ensure that the tensile strength, the elongation at break and the low-temperature flexibility of the coating meet the requirements.
In some embodiments, the modified alkoxysilane-terminated polyether is derived from reacting a hydroxyl terminated polyether with an isocyanate terminated silane coupling agent.
In some embodiments, the alkoxysilane-terminated polyether has the structural formula I,
wherein n is a positive integer, R comprises at least one of methyl and methoxy, R 1 、R 2 Independently represents a C1-C4 alkylene group, and the dynamic viscosity of the alkoxysilane-terminated polyether is 30000-60000 mPa.s.
In some embodiments, the polyisocyanate includes at least one of toluene diisocarboxylate, diphenylmethane-4, 4' -diisocyanate, isophorone diisocyanate, dicyclohexylmethane diisocyanate, hexamethylene diisocyanate, lysine diisocyanate, xylylene diisocyanate, tetramethyl isophthalene diisocyanate, triphenylmethane triisocyanate, and 2-lysine triisocyanate.
In some embodiments, the chain extender comprises at least one of TDMA-HY09, 4' -methylenebis (2-chloroaniline), dimethylthiotoluene diamine, diethyltoluene diamine, methylcyclohexane diamine, 4' -methylenebis (3-chloro-2, 6-diethylaniline), and 4,4' -di-sec-butylamino-diphenyl-methane.
In some embodiments, the plasticizer comprises at least one of a trioctyl phosphate plasticizer, a citrate plasticizer, and a phthalate plasticizer.
In some embodiments, the filler comprises at least one of hydrophilic silica, nano calcium carbonate, calcined kaolin, modified calcined kaolin, and carbon black.
In some embodiments, the coupling agent comprises at least one of gamma- (2, 3-glycidoxy) propyltrimethoxysilane, gamma-aminopropyltriethoxysilane, gamma- (beta-aminoethyl) aminopropyltrimethoxysilane, aniline methyltrimethoxysilane, gamma- (2, 3-glycidoxy) propyltriethoxysilane, ureidopropyltrimethoxysilane, and ureidopropyltriethoxysilane.
In some embodiments, the filler is a modified calcined kaolin clay and a hydrophilic silica in a mass ratio of 1:0.25 to 1, wherein the modified calcined kaolin clay is a modified calcined kaolin clay model XJT-3000D.
In some embodiments, the silane-modified polyether waterproof coating further comprises a water scavenger: 16-23 parts of water scavenger comprising at least one of vinyl trimethoxy silane, vinyl triacetoxy silane and vinyl triethoxy silane.
In some embodiments, the silane-modified polyether waterproof coating further comprises a catalyst: 3-5 parts of catalyst comprising at least one of dibutyl tin dilaurate, stannous octoate, dibutyl tin diacetate and chelated tin catalyst.
In some embodiments, the silane-modified polyether waterproof coating further comprises an antioxidant: 5-8 parts of an antioxidant comprising at least one of an antioxidant-1010, an antioxidant-1076, an antioxidant-3114, an antioxidant-168 and an antioxidant-626.
In a second aspect, the present application provides a method for preparing a silane-modified polyether waterproofing coating comprising the steps of:
s10: providing a raw material in the silane-modified polyether waterproof coating according to any one of the embodiments of the first aspect;
s20: and uniformly mixing the raw materials to obtain the silane modified polyether waterproof coating.
In some embodiments, the step S20 specifically includes:
s21: pre-reacting the modified alkoxy silane group end capped polyether, polyisocyanate and chain extender in a plasticizer to obtain a prepolymer;
s22: and uniformly mixing the prepolymer with the rest of raw materials to obtain the silane modified polyether waterproof coating.
In some embodiments, the step S21 specifically includes:
adding modified alkoxy silane end capped polyether into plasticizer, heating to 90-100 deg.c, adding polyisocyanate and reaction for 3-4 hr; cooling to 70-80 ℃ after the reaction is finished, adding a chain extender, and reacting for 1-2 h to obtain the prepolymer.
In a third aspect, the present application provides a waterproof article comprising a substrate, and a waterproof coating layer formed from the silane-modified polyether waterproof coating material according to any one of the embodiments of the first aspect or the silane-modified polyether waterproof coating material prepared by the method according to any one of the embodiments of the second aspect.
Detailed Description
Each example or embodiment in this specification is described in a progressive manner, each example focusing on differences from other examples.
In the description of the present specification, reference to the terms "one embodiment," "some embodiments," "illustrative embodiments," "examples," "specific examples," or "some examples," etc., means that a particular feature, structure, material, or characteristic described in connection with the embodiment or example is included in at least one embodiment or example of the present application. In this specification, schematic representations of the above terms do not necessarily refer to the same embodiments or examples. Furthermore, the particular features, structures, materials, or characteristics described may be combined in any suitable manner in any one or more embodiments or examples.
Furthermore, the terms "first," "second," and the like, are used for descriptive purposes only and are not to be construed as indicating or implying a relative importance or implicitly indicating the number of technical features indicated. Thus, a feature defining "a first" or "a second" may explicitly or implicitly include at least one such feature. In the description of the present application, the meaning of "plurality" is at least two, such as two, three, etc., unless explicitly defined otherwise.
As described in the background art above, the silane modified polyether waterproof coating has the advantages of high elongation, high tensile strength, good low-temperature flexibility, low water absorption and the like, but has low tearing strength, and the formed coating is easy to damage, so that the coating seeps water, and further the phenomena of falling off, stripping and the like occur.
Aiming at the problems, the silane modified polyether waterproof coating is generally used in the scenes with relatively mild use environments such as indoors and the like in the related art, such as kitchen and bathroom, balcony and the like, and when the silane modified polyether waterproof coating is used in the scenes with relatively severe use environments such as roof, outer wall and the like, a certain protection layer is required to be further applied on the basis of the silane modified polyether waterproof coating so as to protect the silane modified polyether waterproof coating from being torn easily, and the service life of the coating is prolonged. Obviously, when used in a scene with a relatively severe use environment, the use of the silane modified polyether waterproof coating to form a waterproof coating clearly increases the construction cost of the waterproof coating significantly.
Based on the above, the application provides the silane modified polyether waterproof coating, and the modified alkoxy silane group end capped polyether with a secondary amine group is used, and is matched with the polyisocyanate and the chain extender, so that the tear strength of the coating can be improved by improving the crosslinking density of the polymer, and the application scene of the silane modified polyether waterproof coating can be effectively expanded. The following provides a detailed description of specific embodiments of the present application.
In a first aspect, the application provides a silane modified polyether waterproof coating, which comprises the following raw materials in parts by mass:
modified alkoxysilane-terminated polyether: 100 parts of modified alkoxy silane end capped polyether containing secondary amino;
alkoxysilane-terminated polyethers: 350-700 parts of alkoxy silane group end capped polyether which does not contain amino groups;
polyisocyanates: 7-16 parts;
chain extender: 27-54 parts;
and (3) a plasticizer: 500-800 parts;
and (3) filling: 300-480 parts;
coupling agent: 35-50 parts.
According to the application, in the silane modified polyether waterproof coating, the modified alkoxy silane group end capped polyether contains secondary amine groups, the secondary amine groups have reactivity with polyisocyanate, a cross-linked network structure can be formed under the action of a chain extender, the modified alkoxy silane group end capped polyether reacts with the polyisocyanate to be connected through urea bonds, the existence of the urea bonds can improve the crystallinity of chain segments to a certain extent, the improvement of the tearing performance of the coating is facilitated, in addition, the alkoxy silane group end capped polyether which is not reactive with the polyisocyanate is inserted into the cross-linked network structure in a straight chain segment mode at the same time, the flexibility of the coating is maintained, and the obtained coating has good tearing strength, and meanwhile, the other performances of the silane modified polyether waterproof coating are not remarkably deteriorated, and still has good tensile strength, elongation at break, cohesiveness and low-temperature flexibility.
Specifically, based on 100 parts of modified alkoxy silane-based end-capped polyether, 7-16 parts of polyisocyanate and 27-54 parts of chain extender are used in the coating to form a good cross-linked network structure, the tearing strength of the coating is improved, 350-700 parts of alkoxy silane-based end-capped polyether is used for enabling the coating to have good tensile strength, elongation at break, cohesiveness and low-temperature flexibility, 500-800 parts of plasticizer can be used for enabling the coating to have good workability by improving the viscosity and fluidity of the coating, meanwhile, the flexibility of the coating can be improved, 300-480 parts of filler is beneficial to further improving the tensile strength and the tearing strength of the coating, meanwhile, the production cost of the coating can be reduced, and 35-50 parts of coupling agent can be used for enabling all components in the coating to be dispersed more uniformly, improving the stability of the coating and improving the cohesiveness of the coating.
In addition, the alkoxysilane-terminated polyether has a meaning well known in the art, and specifically refers to a polymer that is terminated with an alkoxysilane group and takes polyether as a long chain.
In some embodiments, the alkoxysilane-terminated polyether is 400 to 650 parts by mass, and the resulting coating can further improve the adhesion properties of the coating while ensuring tear strength.
In some embodiments, the modified alkoxysilane-terminated polyether is derived from reacting a hydroxyl terminated polyether with an isocyanate terminated silane coupling agent.
In some embodiments, the structure of the modified alkoxy silane group end capped polyether is specifically limited, the modified silane coupling agent comprises isocyanate groups, the modified alkoxy silane group end capped polyether is bonded with hydroxyl groups of polyether end groups, the silane coupling agent is grafted at two ends of the polyether through carbamate groups, and meanwhile, the secondary amine groups on the carbamate groups have reactivity with polyisocyanate, so that a coating formed by the paint has good tearing strength.
In some embodiments, the dynamic viscosity of the modified alkoxysilane-terminated polyether can be 10000 to 30000 mpa.s.
In some embodiments, the modified alkoxysilane-terminated polyether includesSTP-E10、STP-E15、/>STP-E30 and->At least one of STP-E35.
In some of the above embodiments, the types of modified siloxy-terminated polyethers are specifically defined, and it is understood that the modified alkoxysilane-terminated polyethers are not limited to the above, and those skilled in the art can select other types of modified alkoxysilane-terminated polyethers containing amine groups according to actual needs. As an example, one embodiment of the present application uses a material available from Yu Wake chemical (china) limitedSTP-E35 was used as modified alkoxysilane-terminated polyether with a dynamic viscosity of about 30000 mPa.s.
In some embodiments, the alkoxysilane-terminated polyether has the structural formula I,
wherein n is a positive integer, R comprises at least one of methyl and methoxy, R 1 、R 2 Independently represents a C1-C4 alkylene group, and the dynamic viscosity of the alkoxysilane-terminated polyether is 30000-60000 mPa.s.
In some of the embodiments described above, the structure and viscosity of the alkoxysilane-terminated polyether are specifically defined, which are not reactive with polyisocyanates, allowing the coating to be formed with good tensile strength, elongation at break, adhesion, and low temperature flexibility. Wherein C1-C4 alkylene represents a straight-chain or branched alkylene group having 1 to 4 carbon atoms.
The dynamic viscosity of the modified alkoxysilane-terminated polyether and the alkoxysilane-terminated polyether is related to the molecular weight of the alkoxysilane-terminated polyether, i.e., the molecular weight of the modified alkoxysilane-terminated polyether and the alkoxysilane-terminated polyether can be confirmed by limiting the dynamic viscosity of the modified alkoxysilane-terminated polyether and the alkoxysilane-terminated polyether; dynamic viscosity has a meaning well known in the art and can be determined according to methods and instruments known in the art, for example, by reference to the GB/T10247-2008 viscosity measurement method.
In some embodiments, the alkoxysilane-terminated polyether includes MSSAX227、MSSAX327、MS/>SAX220 and MS->At least one of SAX 750.
In some of the above embodiments, the types of alkoxysilane-terminated polyethers are specifically defined, and it is understood that the alkoxysilane-terminated polyethers are not limited to the above, and those skilled in the art can select other types of alkoxysilane-terminated polyethers having a long chain of polyether and having an alkoxysilane group as desired. As an example, in one embodiment of the present application, MS from a clock trade (Shanghai) Limited is usedSAX750 as an alkoxysilane-terminated polyether has a dynamic viscosity of about 35000 mPa.s.
In some embodiments, the polyisocyanate comprises at least one of toluene diiso-ate, diphenylmethane-4, 4' -diisocyanate, isophorone diisocyanate, dicyclohexylmethane diisocyanate, hexamethylene diisocyanate, lysine diisocyanate, xylylene diisocyanate, tetramethyl isophthalene diisocyanate, triphenylmethane triisocyanate, and 2-lysine triisocyanate.
In some of the above embodiments, the types of polyisocyanates are specifically defined, and it is understood that the polyisocyanates have the meaning well known in the art, and refer to a class of compounds having two or more isocyanate groups, and it is understood that the polyisocyanates are not limited to the above, and those skilled in the art can select other types of polyisocyanates having two or more isocyanate groups according to actual needs. As an example, triphenylmethane triisocyanate available from new materials inc, hubei, in one embodiment of the present application is used.
In some embodiments, the chain extender comprises at least one of TDMA-HY09, 4' -methylenebis (2-chloroaniline), dimethylthiotoluene diamine, diethyltoluene diamine, methylcyclohexane diamine, 4' -methylenebis (3-chloro-2, 6-diethylaniline), and 4,4' -di-sec-butylamino-diphenyl-methane.
In some of the above embodiments, the types of the chain extender are specifically limited, and the chain extender is mainly diamine or diol compounds, so that molecular chains can be extended and molecular weight can be increased, and a coating formed by the paint has higher tearing strength. It will be appreciated that the chain extender is not limited to the above, and those skilled in the art can select chain extenders known in the art to be useful in polyurethane reactions according to actual needs. As an example, in one embodiment of the present application using TDMA-HY09 available from Guangzhou Yourun synthetic materials Co., ltd and dimethyl thiotoluenediamine (DMTDA) available from Zhang Kong Chemie Co., ltd as chain extenders, the mass ratio of TDMA-HY09 to DMTDA may be 1:0.2 to 1.
In some embodiments, the plasticizer comprises at least one of a trioctyl phosphate plasticizer, a citrate plasticizer, and a phthalate plasticizer.
In some of the above embodiments, the kind of plasticizer is specifically defined, and it is understood that the plasticizer is not limited to the above ones, and those skilled in the art can select plasticizers known in the art to be useful for coating according to actual needs. As an example, diisodecyl phthalate, available from shanghai meyer chemical technology limited, is used as a plasticizer in one embodiment of the present application.
In some embodiments, the filler comprises at least one of hydrophilic silica, nano calcium carbonate, calcined kaolin, modified calcined kaolin, and carbon black.
In some of the above embodiments, the kind of filler is specifically defined, and it is understood that the filler is not limited to the above, and those skilled in the art can select a filler known in the art to be usable for a paint according to actual needs.
In some embodiments, the coupling agent includes at least one of gamma- (2, 3-glycidoxy) propyltrimethoxysilane, gamma-aminopropyl triethoxysilane, gamma- (beta-aminoethyl) aminopropyl trimethoxysilane, aniline methyltrimethoxysilane, gamma- (2, 3-glycidoxy) propyltriethoxysilane, ureidopropyltrimethoxysilane, and ureidopropyltriethoxysilane.
In some of the above embodiments, the kind of the coupling agent is specifically defined, and it is understood that the coupling agent is not limited to the above, and those skilled in the art can select a coupling agent known in the art to be useful for coating according to actual needs. As an example, aniline methyltrimethoxysilane is used as a coupling agent in one embodiment of the present application.
In some embodiments, the filler is a modified calcined kaolin clay and a hydrophilic silica in a mass ratio of 1:0.25 to 1, wherein the modified calcined kaolin clay is a modified calcined kaolin clay model XJT-3000D.
In some of the above embodiments, further limiting the types of fillers, the inventors have found that using a mass ratio of modified calcined kaolin and hydrophilic silica of 1:0.25 to 1 as fillers results in a coating having a higher tear strength than using a typical filler. As an example, in an embodiment of the present application, a mass ratio of 1:0.25 to 1 of modified calcined kaolin with model XJT-3000D from Shanxi Jintai technology Co., ltd and hydrophilic fumed silica with model De solid AEROSIL 380 from Guangzhou Yirui New material Co., ltd.
In some embodiments, the silane-modified polyether waterproof coating further comprises a water scavenger: 16-23 parts of a water scavenger comprising at least one of vinyl trimethoxy silane, vinyl triacetoxy silane and vinyl triethoxy silane.
In some embodiments, the silane-modified polyether waterproof coating may further comprise a water scavenger, it being understood that the alkoxysilane-based terminated polyether in the silane-modified polyether waterproof coating is hydrolyzed and cured in water, so 16 to 23 parts of the water scavenger may be added in order to improve the processing and storage stability of the silane-modified polyether waterproof coating, it being understood that the water scavenger is not limited to the above, and those skilled in the art may select the water scavenger known in the art to be useful for coating according to actual needs. As an example, vinyltriacetoxysilane is used as the water scavenger in one embodiment of the present application.
In some embodiments, the silane-modified polyether waterproof coating further comprises a catalyst: 3-5 parts of catalyst comprising at least one of dibutyl tin dilaurate, stannous octoate, dibutyl tin diacetate and chelated tin catalyst.
In some of the above embodiments, the silane-modified polyether waterproof coating may further include a catalyst which may further increase the crosslinking curing rate to reduce the construction time, so that 3 to 5 parts of the catalyst may be added to the waterproof coating, it being understood that the catalyst is not limited to the above, and a person skilled in the art may select a catalyst known in the art to be useful for crosslinking polyurethane according to actual needs. As an example, tin chelate U303, available from Guangzhou, inc. of firm chemical industry, inc., is used as a catalyst in one embodiment of the present application.
In some embodiments, the silane-modified polyether waterproof coating further comprises an antioxidant: 5-8 parts of an antioxidant comprising at least one of an antioxidant-1010, an antioxidant-1076, an antioxidant-3114, an antioxidant-168 and an antioxidant-626.
In some embodiments, the silane modified polyether waterproof coating can further comprise an antioxidant, and the antioxidant can prevent organic components in the coating from oxidative degradation, so that the durability and durability of the coating can be effectively improved, and the service life of the coating can be prolonged, and therefore 5-8 parts of the antioxidant can be added into the waterproof coating. It will be appreciated that the antioxidant is not limited to the above, and those skilled in the art can select an antioxidant known in the art to be useful for coating materials according to actual needs. As an example, antioxidant-1010 is used as an antioxidant in an embodiment of the present application.
In a second aspect, the present application provides a method for preparing a silane-modified polyether waterproofing coating comprising the steps of:
s10: providing a raw material in the silane-modified polyether waterproof coating according to any one of the embodiments of the first aspect;
s20: and uniformly mixing the raw materials to obtain the silane modified polyether waterproof coating.
According to the present application, the silane-modified polyether waterproof coating material prepared by using the raw materials in the silane-modified polyether waterproof coating material of any one of the embodiments of the first aspect has the advantageous effects of the first aspect.
In some embodiments, step S20 specifically includes:
s21: pre-reacting modified alkoxy silane end capped polyether, polyisocyanate and a chain extender in a plasticizer to obtain a prepolymer;
s22: and uniformly mixing the prepolymer and the rest raw materials to obtain the silane modified polyether waterproof coating.
In some embodiments, the specific steps of uniformly mixing the raw materials are further limited, the modified alkoxysilane-terminated polyether, the polyisocyanate and the chain extender can be pre-reacted in the plasticizer to form a prepolymer, and then the prepolymer and the rest raw materials are uniformly mixed, so that the curing rate of the coating is improved, and meanwhile, the formation of the prepolymer is more favorable for the formation of a crosslinked network, so that the tearing strength of the coating is further improved.
In some embodiments, step S21 specifically includes:
adding modified alkoxy silane end capped polyether into plasticizer, heating to 90-100 deg.c, adding polyisocyanate and reaction for 3-4 hr; cooling to 70-80 ℃ after the reaction is finished, adding a chain extender, and reacting for 1-2 h to obtain the prepolymer.
In some of the above embodiments, the specific process of forming the prepolymer is further defined by reacting the modified alkoxysilane-terminated polyether with the polyisocyanate using the plasticizer as a solvent, and then adding the chain extender to further extend the chain segment and crosslink, which facilitates the formation of a prepolymer of suitable molecular weight, thereby further improving the tear strength of the coating.
As an example, the silane-modified polyether waterproof paint can be prepared by the following steps:
adding modified alkoxy silane end capped polyether and dehydrated plasticizer into a reaction kettle;
under the stirring condition, heating the reaction kettle to 90-100 ℃, adding polyisocyanate, and reacting for 3-4 hours at constant temperature;
cooling the reaction kettle to 70-80 ℃, adding a chain extender, and reacting at constant temperature for 1-2 h to obtain a prepolymer;
cooling the reaction kettle to 60-70 ℃, adding alkoxy silane-based capped polyether, adding dehydrated filler and antioxidant under the stirring condition, and vacuumizing and stirring the reaction kettle for 1-2 hours until the slurry is uniformly dispersed;
cooling the reaction kettle to 50-60 ℃, adding a water removing agent and a coupling agent, and vacuumizing and stirring the reaction kettle for 0.5-1 h;
maintaining the temperature of the reaction kettle at 50-60 ℃, adding a catalyst, and vacuumizing and stirring the reaction kettle for 0.5-1 h;
and cooling the reaction kettle to below 50 ℃, and discharging under the protection of nitrogen to obtain the silane modified polyether waterproof coating.
In a third aspect, the present application provides a water-repellent article comprising a substrate, and a water-repellent coating formed from the silane-modified polyether water-repellent coating according to any one of the embodiments of the first aspect or the silane-modified polyether water-repellent coating prepared according to the method of any one of the embodiments of the second aspect.
According to the present application, the waterproof article comprises a waterproof coating layer formed of the silane-modified polyether waterproof coating according to any one of the embodiments of the first aspect or the silane-modified polyether waterproof coating prepared according to any one of the embodiments of the second aspect, and thus the advantageous effects of the first aspect and the second aspect.
Hereinafter, embodiments of the present application are described. The embodiments described below are exemplary only for the purpose of illustrating the present application and are not to be construed as limiting the present application. The examples are not to be construed as limiting the specific techniques or conditions described in the literature in this field or as per the specifications of the product. The reagents or apparatus used were conventional products commercially available without the manufacturer's attention.
Example 1
Preparation of silane modified polyether waterproof paint:
the raw materials with the following mass parts are provided:
STP-E35:20 parts;
SAX750:85 parts;
diisodecyl phthalate: 105 parts;
triphenylmethane triisocyanate: 3 parts;
TDMA-HY09:4.6 parts;
DMTDA:1.5 parts;
XJT-3000D:46 parts;
AEROSIL 380:18 parts;
antioxidant-1010: 1 part;
vinyl triacetoxy silane: 3 parts;
aniline methyltrimethoxysilane: 8 parts;
chelate tin U303:1.4 parts.
STP-E35 and dehydrated diisodecyl phthalate are added into a reaction kettle;
under the stirring condition, heating the reaction kettle to 90-100 ℃, adding triphenylmethane triisocyanate, and reacting for 3-4 hours at constant temperature;
cooling the reaction kettle to 70-80 ℃, adding TDMA-HY09 and DMTDA, and reacting at constant temperature for 1-2 h to obtain prepolymer;
cooling the reaction kettle to 60-70 ℃, adding SAX750, adding dehydrated XJT-3000D, AEROSIL and antioxidant-1010 under stirring, and vacuumizing and stirring the reaction kettle for 1-2 hours until the slurry is uniformly dispersed;
cooling the reaction kettle to 50-60 ℃, adding vinyl triacetoxy silane and aniline methyl trimethoxy silane, and vacuumizing and stirring the reaction kettle for 0.5-1 h;
maintaining the temperature of the reaction kettle at 50-60 ℃, adding the chelated tin U303, and vacuumizing and stirring the reaction kettle for 0.5-1 h; and cooling the reaction kettle to below 50 ℃, and discharging under the protection of nitrogen to obtain the silane modified polyether waterproof coating.
Example 2
Preparation of silane modified polyether waterproof paint:
the preparation process is substantially the same as in example 1, except that the raw materials are different in mass parts, specifically: STP-E35:18 parts;
SAX750:88 parts;
diisodecyl phthalate: 101 parts;
triphenylmethane triisocyanate: 3 parts;
TDMA-HY09:4.6 parts;
DMTDA:1.5 parts;
XJT-3000D:44 parts;
AEROSIL 380:21 parts;
antioxidant-1010: 1 part;
vinyl triacetoxy silane: 3 parts;
aniline methyltrimethoxysilane: 8 parts;
chelate tin U303:1.2 parts.
Example 3
Preparation of silane modified polyether waterproof paint:
the preparation process is substantially the same as in example 1, except that the raw materials are different in mass parts, specifically: STP-E35:25 parts;
SAX750:80 parts;
diisodecyl phthalate: 105 parts;
triphenylmethane triisocyanate: 3.6 parts;
TDMA-HY09:4.8 parts;
DMTDA:1.6 parts;
XJT-3000D:45 parts;
AEROSIL 380:20 parts;
antioxidant-1010: 1 part;
vinyl triacetoxy silane: 3 parts;
aniline methyltrimethoxysilane: 7.6 parts;
chelate tin U303:1.3 parts.
Example 4
Preparation of silane modified polyether waterproof paint:
the procedure was substantially the same as in example 1, except that XJT-3000D was used in place of AEROSIL 380 in the same parts by mass.
Example 5
Preparation of silane modified polyether waterproof paint:
the preparation procedure was substantially the same as in example 1, except that the same mass parts of AEROSIL 380 was used instead of XJT-3000D.
Example 6
Preparation of silane modified polyether waterproof paint:
the preparation process is substantially the same as in example 1, except that the same mass part of nano calcium carbonate is used instead of XJT-3000D.
Example 7
Preparation of silane modified polyether waterproof paint:
the procedure was substantially as in example 1, except that SAX750 parts by weight was 75 parts.
Example 8
Preparation of silane modified polyether waterproof paint:
the procedure was substantially as in example 1, except that SAX750 parts by weight was 140 parts.
Comparative example 1
Preparation of silane modified polyether waterproof paint:
the preparation was the same as in example 1, except that triphenylmethane triisocyanate, TDMA-HY09 and DMYDA were not added.
Comparative example 2
Preparation of silane modified polyether waterproof paint:
the preparation was substantially the same as in example 1, except that the same mass parts of SAX750 were used instead of STP-E35.
Test mode
The silane-modified polyether waterproof coatings obtained in examples 1 to 8 and comparative examples 1 and 2 were subjected to performance test by the following methods:
the surface drying time, the actual drying time, the tensile strength, the elongation at break, the bonding strength, the low-temperature bending property and the water impermeability of the silane modified polyether waterproof coating are tested by referring to T/CBMF 105-2021 and T/CWA 203-2021; the tearing strength of the silane modified polyether waterproof paint is tested by referring to GB/T16777-2008; the test results are shown in Table 1.
TABLE 1
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As can be seen from table 1, the tear strength and the bonding strength of the waterproof coating obtained in each example are obviously improved compared with those of the comparative examples, so that the durability of the coating can be effectively improved; meanwhile, other properties of the waterproof coating can meet related requirements, and other properties of the silane modified polyether waterproof coating are not obviously deteriorated. In comparative examples 1 and 2, the modified alkoxysilane-terminated polyether cannot be reacted with polyisocyanate to form a crosslinked network structure, and thus the tear strength is low.
According to examples 1 to 6, the types of the fillers in the silane-modified polyether waterproof coating also have a certain influence on the performance of the coating, and when the specific modified calcined kaolin and the hydrophilic silica are selected to be used as the fillers in a certain proportion, the tear strength of the silane-modified polyether waterproof coating is obviously improved compared with other fillers, and the other performances of the silane-modified polyether waterproof coating are not influenced.
It is understood from examples 1, 7 and 8 that the ratio of the modified alkoxysilane-terminated polyether to the alkoxysilane-terminated polyether in the silane-modified polyether waterproof coating material also has a certain effect on the performance of the coating material, and that the adhesive strength of the coating material is higher when the alkoxysilane-terminated polyether is 400 to 650 parts based on 100 parts of the modified alkoxysilane-terminated polyether.
Therefore, compared with the common silane modified polyether waterproof coating, the silane modified polyether waterproof coating provided by the application has higher tearing strength, so that the application range of the silane modified polyether waterproof coating can be further expanded.
Finally, it should be noted that: the above embodiments are only for illustrating the technical solution of the present application, and not for limiting the same; although the present application has been described in detail with reference to the foregoing embodiments, it should be understood by those of ordinary skill in the art that: the technical scheme described in the foregoing embodiments can be modified or some or all of the technical features thereof can be replaced by equivalents; such modifications and substitutions do not depart from the spirit of the corresponding technical solutions from the scope of the technical solutions of the embodiments of the present application.

Claims (10)

1. The silane modified polyether waterproof coating is characterized by comprising the following raw materials in parts by mass:
modified alkoxysilane-terminated polyether: 100 parts of modified alkoxy silane end capped polyether containing secondary amino;
alkoxysilane-terminated polyethers: 350-700 parts of an alkoxy silane group end capped polyether chain segment does not contain an amino group;
polyisocyanates: 7-16 parts;
chain extender: 27-54 parts;
and (3) a plasticizer: 500-800 parts;
and (3) filling: 300-480 parts;
coupling agent: 35-50 parts.
2. The silane-modified polyether waterproof paint according to claim 1, wherein the modified alkoxysilane-terminated polyether is obtained by reacting polyether having hydroxyl groups as end groups with a silane coupling agent having isocyanate groups as end groups.
3. The silane-modified polyether waterproof paint of claim 1, wherein the structural formula of the alkoxysilane-terminated polyether is shown as formula I,
wherein n is a positive integer, R comprises at least one of methyl and methoxy, R 1 、R 2 Independently represents a C1-C4 alkylene group, and the dynamic viscosity of the alkoxysilane-terminated polyether is 30000-60000 mPa.s.
4. The silane-modified polyether waterproof coating according to claim 1, characterized in that the silane-modified polyether waterproof coating satisfies at least one of the following conditions:
1) The polyisocyanate comprises at least one of toluene diisoacid ester, diphenylmethane-4, 4' -diisocyanate, isophorone diisocyanate, dicyclohexylmethane diisocyanate, hexamethylene diisocyanate, lysine diisocyanate, xylylene diisocyanate, tetramethyl m-xylylene diisocyanate, triphenylmethane triisocyanate and 2-lysine triisocyanate;
2) The chain extender comprises at least one of TDMA-HY09, 4' -methylenebis (2-chloroaniline), dimethyl thiotoluenediamine, diethyl toluenediamine, methyl cyclohexanediamine, 4' -methylenebis (3-chloro-2, 6-diethylaniline) and 4,4' -di-sec-butylamino-diphenyl methane;
3) The plasticizer comprises at least one of trioctyl phosphate plasticizer, citrate plasticizer and phthalate plasticizer;
4) The filler comprises at least one of hydrophilic silica, nano calcium carbonate, calcined kaolin, modified calcined kaolin and carbon black;
5) The coupling agent comprises at least one of gamma- (2, 3-epoxypropoxy) propyl trimethoxysilane, gamma-aminopropyl triethoxysilane, gamma- (beta-aminoethyl) aminopropyl trimethoxysilane, aminomethyl trimethoxysilane, gamma- (2, 3-epoxypropoxy) propyl triethoxysilane, allopropyl trimethoxysilane and allopropyl triethoxysilane.
5. The silane-modified polyether waterproof paint according to claim 1 or 4, wherein the filler is modified calcined kaolin and hydrophilic silica in a mass ratio of 1:0.25-1, wherein the modified calcined kaolin is modified calcined kaolin of model XJT-3000D.
6. The silane-modified polyether waterproof coating of claim 1 or 4, further comprising at least one of the following raw materials:
1) Water scavenger: 16-23 parts of a water scavenger comprising at least one of vinyl trimethoxy silane, vinyl triacetoxy silane and vinyl triethoxy silane;
2) Catalyst: 3-5 parts of catalyst comprising at least one of dibutyl tin dilaurate, stannous octoate, dibutyl tin diacetate and chelated tin catalyst;
3) An antioxidant: 5-8 parts of an antioxidant comprising at least one of an antioxidant-1010, an antioxidant-1076, an antioxidant-3114, an antioxidant-168 and an antioxidant-626.
7. A process for preparing a silane-modified polyether waterproof coating comprising the steps of:
s10: providing a raw material in the silane-modified polyether waterproof coating material according to any one of claims 1 to 6;
s20: and uniformly mixing the raw materials to obtain the silane modified polyether waterproof coating.
8. The method according to claim 7, wherein the step S20 specifically includes:
s21: pre-reacting the modified alkoxy silane group end capped polyether, polyisocyanate and chain extender in a plasticizer to obtain a prepolymer;
s22: and uniformly mixing the prepolymer with the rest of raw materials to obtain the silane modified polyether waterproof coating.
9. The method according to claim 8, wherein the step S21 specifically includes:
adding modified alkoxy silane end capped polyether into plasticizer, heating to 90-100 deg.c, adding polyisocyanate and reaction for 3-4 hr; cooling to 70-80 ℃ after the reaction is finished, adding a chain extender, and reacting for 1-2 h to obtain the prepolymer.
10. A waterproof article comprising a substrate and a waterproof coating layer formed from the silane-modified polyether waterproof coating material according to any one of claims 1 to 6 or the silane-modified polyether waterproof coating material produced by the method according to any one of claims 7 to 9.
CN202311668605.3A 2023-12-06 2023-12-06 Silane modified polyether waterproof coating and preparation method and application thereof Pending CN117701124A (en)

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US20030225235A1 (en) * 2002-05-31 2003-12-04 Roesler Richard R. Moisture-curable, polyether urethanes with reactive silane groups and their use as sealants, adhesives and coatings
CN101993522A (en) * 2009-08-19 2011-03-30 赢创高施米特有限公司 Novel urethane-containing silylated prepolymers and process for preparation thereof
CN107022333A (en) * 2017-04-19 2017-08-08 常熟市恒信粘胶有限公司 Silane-terminated polyether modified structure fluid sealant
CN107880837A (en) * 2017-10-30 2018-04-06 广州市白云化工实业有限公司 Exfoliated silane modified polyether adhesive of shock resistance and preparation method thereof
CN111423837A (en) * 2020-04-08 2020-07-17 上海抚佳精细化工有限公司 TPU hot melt adhesive and preparation method thereof
CN116285618A (en) * 2022-12-20 2023-06-23 蔚湃建筑科技(上海)有限公司 Organosilicon waterproofing agent and preparation method thereof
CN116355377A (en) * 2023-04-04 2023-06-30 中铁建华南建设(广州)高科技产业有限公司 Silane modified polyether resin material, preparation method thereof and grouting material
CN117165159A (en) * 2023-09-26 2023-12-05 科顺防水科技股份有限公司 Silane modified polyether waterproof paint and preparation method thereof

Patent Citations (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20030225235A1 (en) * 2002-05-31 2003-12-04 Roesler Richard R. Moisture-curable, polyether urethanes with reactive silane groups and their use as sealants, adhesives and coatings
CN101993522A (en) * 2009-08-19 2011-03-30 赢创高施米特有限公司 Novel urethane-containing silylated prepolymers and process for preparation thereof
CN107022333A (en) * 2017-04-19 2017-08-08 常熟市恒信粘胶有限公司 Silane-terminated polyether modified structure fluid sealant
CN107880837A (en) * 2017-10-30 2018-04-06 广州市白云化工实业有限公司 Exfoliated silane modified polyether adhesive of shock resistance and preparation method thereof
CN111423837A (en) * 2020-04-08 2020-07-17 上海抚佳精细化工有限公司 TPU hot melt adhesive and preparation method thereof
CN116285618A (en) * 2022-12-20 2023-06-23 蔚湃建筑科技(上海)有限公司 Organosilicon waterproofing agent and preparation method thereof
CN116355377A (en) * 2023-04-04 2023-06-30 中铁建华南建设(广州)高科技产业有限公司 Silane modified polyether resin material, preparation method thereof and grouting material
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